Yield:78-51-3 98%

Reaction Conditions:

with magnesium chloride;trichlorophosphate at 50 - 80; for 5 h;Large scale;Reagent/catalyst;Temperature;

Steps:

1-3; 1-2 Example 1
1. Pump 1540kg (13.03 kilomoles) of ethylene glycol monobutyl ether into the reactor, catalyst 1Kg magnesium chloride was put into the reactor, cool down to 20-25 °C, turn on the vacuum, and add 400 kg (2.61 kmol, the molar ratio of phosphorus oxychloride to ethylene glycol monobutyl ether is 1: 5), after 3 to 5 hours of dropping, the temperature was gradually raised to 50 to 80 ° C after the dropping, and the reaction was kept for 5 hours.
2. After the gas phase detection reaction is complete, switch the vacuum (vacuum degree is 2 4KPa) to distill the ethylene glycol monobutyl ether under reduced pressure, and the temperature for the reduced pressure distillation is 110-120 °C. Gas phase detection of ethylene glycol monobutyl ether (5-10%) content is 6.5%, stop the distillation; the steps of the gas phase detection (the gas phase detection methods involved in the embodiments or comparative examples of the invention adopt the following methods) are as follows: gas phase analysis method: injection temperature: 200 ° C, detector: 220 ° C column temperature:70 , heating up to 280 at 15 °C/min, gas chromatography column: OV-17 capillary chromatography column, 25m * 0.53mm * 0.25um.
Weigh 0.5g of the sample and add 10ml of chloroform to dissolve, and inject 0.2ul. The content of ethylene glycol monobutyl ether was measured.
3. Cool down to 70 80 , slowly add sodium carbonate, adjust PH = 7 8, then, distilled under reduced pressure (vacuum degree is 2~4 KPa), and the remaining ethylene glycol monobutyl ether is distilled off. Distillation temperature to 130 145 , ethylene glycol monobutyl ether content (≤0.1%) 0.08%, the distillation under reduced pressure was stopped to obtain crude tris (butoxyethyl) phosphate.
4. Purification process: The crude product is washed with water, the washing temperature is 55-60 ° C, and the aqueous layer is separated to PH = 7-8. The tris(butoxyethyl)phosphate was washed with water and dehydrated under reduced pressure. The vacuum distillation temperature is 125 to 130 ° C, and the vacuum degree is 8 to 9KPa. 1018 kg of the distilled product was input into the finished storage tank, and the yield was 98%.

References:

Zhejiang Wansheng Co., Ltd.;Wang Qiuwei;Jin Yiping;Niu Lidan CN110357921, 2019, A Location in patent:Paragraph 0047-0087

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